CN102590280A - Gas sensor array based on microwell structure and manufacturing method of gas sensor array - Google Patents

Gas sensor array based on microwell structure and manufacturing method of gas sensor array Download PDF

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CN102590280A
CN102590280A CN2012100527260A CN201210052726A CN102590280A CN 102590280 A CN102590280 A CN 102590280A CN 2012100527260 A CN2012100527260 A CN 2012100527260A CN 201210052726 A CN201210052726 A CN 201210052726A CN 102590280 A CN102590280 A CN 102590280A
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sensor array
gas sensor
little well
organic
little
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谢光忠
蒋亚东
杜晓松
太惠玲
朱涛
周泳
廖剑
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University of Electronic Science and Technology of China
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Abstract

The invention discloses a gas sensor array based on a microwell structure and a manufacturing method of the gas sensor array. The gas sensor array comprises at least four independent sensor units, wherein each sensor unit adopts a microwell structure, a polyimide isolation layer is arranged among microwells; sensitive films consisting of organic films, organic/inorganic composite films or organic-inorganic multilayer films are deposited in the microwells, and interdigital electrodes are arranged on the surfaces of the microwells. The polyimide isolation layer is arranged among the microwells; an electronic polymer sensitive material can be effectively prevented from overflowing and flowing into the adjacent microwells without causing cross pollution of the sensitive materials among the microwells when dropped in one microwell, thus the selectivity and the stability of the sensors are ensured; and meanwhile, the gas sensor array has a simple structure and lower processing cost, and can be widely applied to the fields such as atmospheric environmental monitoring, aerospace sealed cabin air quality detection and food safety.

Description

A kind of gas sensor array based on little well construction and preparation method thereof
Technical field
The present invention relates to microelectromechanical systems gas sensor and electronic polymer sensitive material field, be specifically related to a kind of gas sensor array based on little well construction and preparation method thereof.
Background technology
Analysis to mixed gas is an important step of scientific research, production run and environment measuring.Because gas sensor exists shortcomings such as cross sensitivity, poor selectivity, therefore in mixed gas, be difficult to measure selectively the composition and the content of certain gas.Based on the electric nasus system of gas sensor array and pattern-recognition is the important channel that solves the gas sensor cross-sensitivity, and wherein gas sensor array is the device of core the most in the Electronic Nose Technology.Development along with the MEMS technology applies to Electronic Nose with integrated sensor array, helps miniaturization, the low-power consumption of Electronic Nose.
For a lot of based on the gas sensor kind of MEMS technology, according to the different detection principle, can be divided into: 1) utilize the adsorption mechanism of gas sensitization film, representation type has cantilever beam type, electricity to lead change type and sonic surface wave type; 2) according to the optics and the acoustooptics characteristic of gas self, combine the MEMS structure again and the sensor made, its representation type has spectroscopic methodology and sound and light spectroscopy; 3) utilize the catalytic combustion type detection method to detect flammable explosive gas; 4) adopt High-Field asymmetric waveform ion mobility spectrometry (FAIMS) technology to realize the detection of gas.
According to the difference of sensitive material, gas sensor array mainly contains two big types at present: one type is adopted SnO 2, WO 3As sensitive material, another kind of is to adopt polymeric material or polymer composites as sensitive material Deng inorganic semiconductor.Because the inorganic semiconductor gas sensor array generally need be operated under 300 ℃-500 ℃ the high temperature, power consumption is bigger; And can at room temperature work based on the gas sensor of polymeric material, therefore extensively carried out the research of polymer gas sensor array aspect both at home and abroad.In MEMS electronic polymer gas sensor array field, extensively carried out the research of aspects such as OTFT sensor array, SAW sensor array at present both at home and abroad; But the polymer gas sensor array research to based on little well construction does not appear in the newspapers at present at home as yet, does not have the application of related invention patent, even rarely have report abroad yet yet.People such as calendar year 2001 U.S. Zee Frank adopt micro fabrication to prepare the chemical vapor sensor array based on polymkeric substance, and this array has adopted the little processing structure of body and two kinds of little well constructions of surface micro processing structure; Adopt drop-coating to prepare six kinds of polymkeric substance-carbon black composite sensitive film, at normal temperatures multiple organic molecule is detected; But this array is with single Wei Jing unit simple arrangement together, but not integrated array on the sheet.2005; People such as Korea S Seung-Chul Ha have produced integrated little well construction sensor array on the sheet with 16 independent heating units; They drip eight kinds of different sensitive materials and are coated onto in different little wells; Eight kinds of organic gass are detected, and compared the influence of temperature sensor array sensitivity; But each Wei Jing unit of this sensor array is 2 * 2 mm 2, size is bigger, is unfavorable for the miniaturization and the microminiaturization of system.
Because little well is very little and the spacing adjacent micro well is shorter; When the electronic polymer sensitive material is splashed into one of them little well; Sensitive material usually can overflow and flow to its adjacent little well, causes the cross pollution of sensitive material between different little wells, thereby influences Selectivity of Sensor and stability.
Summary of the invention
To above-mentioned prior art; The technical matters that the present invention will solve is: based on the polymer gas sensor array of little well construction because little well is very little and the spacing of adjacent micro well is short when sensitive material is splashed into one of them little well; Sensitive material usually can overflow and flow to its adjacent little well; Cause the cross pollution of sensitive material between different little wells, influence Selectivity of Sensor and stability.
Technical matters proposed by the invention is to solve like this: a kind of gas sensor array based on little well construction is provided; Comprise at least 4 independently sensor units; It is characterized in that: said sensor unit adopts little well construction, between each little well, is provided with the polyimide separation layer; In said little well well, deposit the sensitive membrane with organic film, organic/inorganic composite film or organic and inorganic multilayer film, little well surface is provided with interdigital electrode.
The length of said little well, width and highly be respectively 550 ~ 650 μ m, 550 ~ 650 μ m and 80 ~ 120 μ m.
Said sensor unit consistency from top to bottom is arranged, and all output electrodes of sensor unit are arranged in a row.
The width of said interdigital electrode, spacing, length and thickness are respectively 50 μ m, 50 μ m, 2000 μ m and 100nm.
The thickness of said polyimide separation layer is 1 ~ 3mm, highly is 200nm ~ 300nm.
The preparation method of above-mentioned a kind of gas sensor array based on little well construction is characterized in that, may further comprise the steps:
Figure 883118DEST_PATH_IMAGE001
adopts the monocrystalline silicon piece of twin polishing as substrate, and the column criterion of going forward side by side is cleaned;
Figure 406504DEST_PATH_IMAGE002
adopts pecvd process to prepare the silicon nitride mask layer on the silicon chip two sides;
Figure 527693DEST_PATH_IMAGE003
carries out photoetching to silicon nitride layer wherein, graphical Wei Jing unit; And carry out dry etching;
Figure 707002DEST_PATH_IMAGE004
adopts KOH solution that silicon chip is carried out wet etching, forms little well;
Figure 982125DEST_PATH_IMAGE005
adopts vacuum vapour deposition at little well surface evaporation metal aluminium (Al) or gold (Au);
Figure 625596DEST_PATH_IMAGE006
carries out photoetching, corrosion to aluminium lamination or gold layer, produces interdigital electrode;
Figure 147713DEST_PATH_IMAGE007
spin-on polyimide on electrode layer; And it is carried out photoetching, produce separation layer;
Figure 876635DEST_PATH_IMAGE008
scribing;
Figure 955449DEST_PATH_IMAGE009
encapsulation;
Figure 391110DEST_PATH_IMAGE010
adopts mask method that location constituency thin film deposition is realized in different Wei Jing unit, and said film is organic thin
Film, organic/inorganic composite film or organic and inorganic multilayer film.
Preparation method according to the gas sensor array based on little well construction provided by the present invention is characterized in that, step 1. in, the silicon chip of employing is 4 inches P types (100) silicon chip of twin polishing, thickness is 450 ~ 550 μ m, resistivity is greater than 1000 Ω cm.
Preparation method according to the gas sensor array based on little well construction provided by the present invention is characterized in that, step 2. in, described silicon nitride medium layer thickness is 700 ~ 800nm.
Preparation method according to the gas sensor array based on little well construction provided by the present invention is characterized in that, in step Described in organic film, organic/inorganic composite film and the organic and inorganic multilayer film, organic phase is polyaniline, polyethylene oxide, gather-the 4-vinylphenol, phthalocyanine complex and polythiophene class, inorganic is nano-TiO mutually 2, In 2O 3, ZnO, SnO 2, CNT etc.; And described film adopt drip be coated with, gas blowout or EFI prepared.
Compared with prior art, the beneficial effect of tool of the present invention shows:
One, the present invention is provided with the polyimide separation layer between each little well; When the electronic polymer sensitive material splashes into one of them little well; Can effectively stop sensitive material to overflow, flow to its adjacent little well; Can not cause the cross pollution of sensitive material between different little wells, thereby guarantee Selectivity of Sensor and stability;
Two, processing technology step of the present invention is simple, and processing cost is lower, and the process-cycle is short, can produce in batches.
Description of drawings
Fig. 1-Fig. 9 is a process flow diagram provided by the present invention;
Figure 10 is the gas sensor array based on little well construction provided by the present invention (no polyimide separation layer) structure vertical view;
Figure 11 is provided by the present invention based on little well construction gas sensor array (containing the polyimide separation layer) structure vertical view;
Reference numeral is: the 1-silicon chip, the 2-silicon nitride, the 3-AZ6112 photoresist, 4-aluminium, 5-AZ6112 photoresist, 6 with the 10-polyimide, 7-composite sensitive film, the little well of 8-, 9-interdigital electrode.
Embodiment
To combine accompanying drawing and embodiment that the present invention is done further description below.
Thought of the present invention is that sensor unit adopts little well construction in based on the gas sensor array of little well construction; Between each little well, be provided with the polyimide separation layer; Stop sensitive material to overflow, flow to its adjacent little well; Can not cause the cross pollution of sensitive material between different little wells, thereby guarantee Selectivity of Sensor and stability.
Like Figure 10 and shown in Figure 11; Figure 10 is the gas sensor array based on little well construction provided by the present invention (no polyimide separation layer) structure vertical view; Figure 11 is provided by the present invention based on little well construction gas sensor array (containing the polyimide separation layer) structure vertical view, and it comprises 4 independently electroded little well sensor units.
Like Fig. 1-shown in Figure 9, making of the present invention is following based on the process flow steps of the gas sensor array of little well construction:
(a) with silicon chip 1 as substrate, it is cleaned, and plates the silicon nitride layer 2 that a layer thickness is about 750nm respectively on the two sides of silicon chip with the PECVD method;
(b) spin coating photoresist AZ6112 on silicon nitride layer 2 therein, obtains having certain thickness AZ6112 glue-line 3 at the rotating speed and the time of control sol evenning machine; Adopt ultraviolet exposure technology, realize of the transfer of mask upper sensor structural sheet figure to AZ6112 glue-line 3; Use developer for positive photoresist that AZ6112 glue-line 3 is developed, obtain having the rectangular window of 600 μ m * 600 μ m;
(c) adopt the RIE dry etching to fall the silicon nitride under the rectangular window, expose silicon chip;
(d) configuration concentration is the KOH solution of 30wt%, and silicon chip is put into wherein, and at 80 ℃ of following wet etching silicon chips, the degree of depth of corrosion back silicon chip window is about 100 μ m;
(e) adopt vacuum vapour deposition having the thick AL layer 4 of plating one deck 100nm on the silicon chip of little well;
(f) spin coating photoresist AZ6112 on AL layer 4, obtains having certain thickness AZ6112 glue-line 5 at the rotating speed and the time of control sol evenning machine; Adopt ultraviolet exposure technology, realize of the transfer of mask upper sensor structural sheet figure to AZ6112 glue-line 5; Use developer for positive photoresist that AZ6112 glue-line 5 is developed;
(g) adopt phosphoric acid in the time of 50 ℃～60 ℃, the AL layer of having handled through step (f) 4 to be corroded, obtain electrode.At this moment the gas sensor array structural drawing based on little well construction that obtains is shown in figure 10;
(h) spin-on polyimide on the silicon chip of handling through above-mentioned steps, obtains the polyimide glue-line 6 that thickness is about 300nm at the rotating speed and the time of control sol evenning machine; Adopt ultraviolet exposure technology, realize of the transfer of mask upper sensor structural sheet figure to AZ6112 glue-line 5 polyimide glue-lines 6; Use developer for positive photoresist that polyimide glue-line 6 is developed, obtain polyimide " enclosure wall ".Then silicon chip is carried out scribing and encapsulation;
(i) having under the mask condition, adopting gas blowout technology to carry out the preparation of organic and inorganic multilayer film, obtaining composite sensing rete 7.
The gas sensor array structural drawing based on little well construction through above-mentioned technology is made is shown in figure 11, and the area of whole sensor array is 12 * 12mm 2

Claims (9)

1. the gas sensor array based on little well construction comprises at least 4 independently sensor units, and it is characterized in that: said sensor unit adopts little well construction, between each little well, is provided with the polyimide separation layer; In said little well well, deposit the sensitive membrane that constitutes with organic film, organic/inorganic composite film or organic and inorganic multilayer film, little well surface is provided with interdigital electrode.
2. the gas sensor array based on little well construction according to claim 1 is characterized in that, the length of said little well, width and highly be respectively 550 ~ 650 μ m, 550 ~ 650 μ m and 80 ~ 120 μ m.
3. the gas sensor array based on little well construction according to claim 1 is characterized in that, said sensor unit consistency from top to bottom is arranged, and all output electrodes of sensor unit are arranged in a row.
4. the gas sensor array based on little well construction according to claim 1 is characterized in that, the width of said interdigital electrode, spacing, length and thickness are respectively 50 μ m, 50 μ m, 2000 μ m and 100nm.
5. the gas sensor array based on little well construction according to claim 1 is characterized in that, the thickness of said polyimide separation layer is 1 ~ 3mm, highly is 200nm ~ 300nm.
6. the preparation method based on the gas sensor array of little well construction is characterized in that, may further comprise the steps:
Figure 2012100527260100001DEST_PATH_IMAGE001
adopts the monocrystalline silicon piece of twin polishing as substrate, and the column criterion of going forward side by side is cleaned;
Figure 994331DEST_PATH_IMAGE002
adopts pecvd process to prepare the silicon nitride mask layer on the silicon chip two sides;
carries out photoetching to silicon nitride layer wherein, graphical Wei Jing unit; And carry out dry etching;
Figure 711751DEST_PATH_IMAGE004
adopts KOH solution that silicon chip is carried out wet etching, forms little well;
Figure 2012100527260100001DEST_PATH_IMAGE005
adopts vacuum vapour deposition at little well surface evaporation metal aluminium Al or golden Au;
Figure 549038DEST_PATH_IMAGE006
carries out photoetching, corrosion to aluminium lamination or gold layer, produces interdigital electrode;
Figure 2012100527260100001DEST_PATH_IMAGE007
spin-on polyimide on electrode layer; And it is carried out photoetching, produce separation layer;
Figure 363410DEST_PATH_IMAGE008
scribing;
Figure 2012100527260100001DEST_PATH_IMAGE009
encapsulation;
Figure 123556DEST_PATH_IMAGE010
adopts mask method that location constituency thin film deposition is realized in different Wei Jing unit, and said film is organic thin
Film, organic/inorganic composite film or organic and inorganic multilayer film.
7. the preparation method of the gas sensor array based on little well construction according to claim 6 is characterized in that, step 1. in, the silicon chip of employing is 4 inches P type silicon chips of twin polishing, thickness is 450 ~ 550 μ m, resistivity is greater than 1000 Ω cm.
8. the preparation method of the gas sensor array based on little well construction according to claim 6 is characterized in that, step 2. in, described silicon nitride layer thickness is 700 ~ 800nm.
9. the preparation method of the gas sensor array based on little well construction according to claim 6 is characterized in that, in step
Figure 328272DEST_PATH_IMAGE010
Described in organic film, organic/inorganic composite film and the organic and inorganic multilayer film, organic phase is polyaniline, polyethylene oxide, gather-the 4-vinylphenol, phthalocyanine complex and polythiophene class, inorganic is nano-TiO mutually 2, In 2O 3, ZnO, SnO 2, CNT etc.; And described film adopt drip be coated with, gas blowout or EFI prepared.
CN2012100527260A 2012-03-02 2012-03-02 Gas sensor array based on microwell structure and manufacturing method of gas sensor array Pending CN102590280A (en)

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Cited By (10)

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CN102759551A (en) * 2012-08-09 2012-10-31 电子科技大学 Perforated plate capacitor type gas sensor and preparation method
CN103529120A (en) * 2013-10-25 2014-01-22 中国电子科技集团公司第三十八研究所 Device and process for preparing composite sensitive film of surface acoustic wave sensor
CN103575612A (en) * 2013-09-17 2014-02-12 中安高科检测科技（北京）有限公司 Preparation method of gas-sensitive sensor array for detecting Xuanwei ham
CN103575611A (en) * 2013-09-17 2014-02-12 中安高科检测科技（北京）有限公司 Preparation method of gas-sensitive sensor array for detecting Cantonese cured meat
CN104952630A (en) * 2015-07-23 2015-09-30 武汉理工大学 Mini-sized supercapacitor with high flexibility and high transparency and large-scale preparation method of mini-sized supercapacitor
CN105181754A (en) * 2015-06-29 2015-12-23 电子科技大学 Compensation type resistor type integrated gas sensor array and preparation method thereof
CN105842290A (en) * 2016-03-24 2016-08-10 山东大学 Inorganic/organic composited gas sensor vacuum on-situ composition method for improving performances of gas sensor
CN106478946A (en) * 2016-10-31 2017-03-08 南京林业大学 The polyaniline of a kind of degradable/porous silicon nano composite material and its preparation method and application
CN108414581A (en) * 2017-02-09 2018-08-17 北京市劳动保护科学研究所 A kind of mini type multiple dimension sensor and manufacturing method
CN110702642A (en) * 2019-10-29 2020-01-17 西南大学 Preparation method of micro-well structured SPRi chip, product and application thereof

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102759551A (en) * 2012-08-09 2012-10-31 电子科技大学 Perforated plate capacitor type gas sensor and preparation method
CN103575611A (en) * 2013-09-17 2014-02-12 中安高科检测科技（北京）有限公司 Preparation method of gas-sensitive sensor array for detecting Cantonese cured meat
CN103575612A (en) * 2013-09-17 2014-02-12 中安高科检测科技（北京）有限公司 Preparation method of gas-sensitive sensor array for detecting Xuanwei ham
CN103529120B (en) * 2013-10-25 2016-06-01 中国电子科技集团公司第三十八研究所 The preparation technology of composite sensitive film of surface acoustic wave sensor
CN103529120A (en) * 2013-10-25 2014-01-22 中国电子科技集团公司第三十八研究所 Device and process for preparing composite sensitive film of surface acoustic wave sensor
CN105181754A (en) * 2015-06-29 2015-12-23 电子科技大学 Compensation type resistor type integrated gas sensor array and preparation method thereof
CN104952630A (en) * 2015-07-23 2015-09-30 武汉理工大学 Mini-sized supercapacitor with high flexibility and high transparency and large-scale preparation method of mini-sized supercapacitor
CN105842290A (en) * 2016-03-24 2016-08-10 山东大学 Inorganic/organic composited gas sensor vacuum on-situ composition method for improving performances of gas sensor
CN105842290B (en) * 2016-03-24 2018-07-03 山东大学 A kind of vacuum in situ complex method for the inorganic-organic hybrid gas sensor for being used to improve gas sensor performance
CN106478946A (en) * 2016-10-31 2017-03-08 南京林业大学 The polyaniline of a kind of degradable/porous silicon nano composite material and its preparation method and application
CN106478946B (en) * 2016-10-31 2018-09-25 南京林业大学 A kind of degradable polyaniline/porous silicon nanocomposite and its preparation method and application
CN108414581A (en) * 2017-02-09 2018-08-17 北京市劳动保护科学研究所 A kind of mini type multiple dimension sensor and manufacturing method
CN110702642A (en) * 2019-10-29 2020-01-17 西南大学 Preparation method of micro-well structured SPRi chip, product and application thereof
CN110702642B (en) * 2019-10-29 2022-03-18 西南大学 Preparation method of micro-well structured SPRi chip, product and application thereof

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Application publication date: 20120718